Analysis of Pesticides

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European Reference Laboratory - FV
Analysis of pesticides in herbs

by GC-QqQ and LC-QqQ
Amadeo R. Fernández-Alba
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Introduction
• In some cultures herbs have been used as a popular beverages for
centuries. Increased interest in those beverages has resulted from
perceived health benefits that may be associated with their
consumption.
• The EFSA annual report of 2008 revealed that:

– 5.8% and 4.5% of the tea and herbs samples, respectively, contained
more than 5 pesticides, one of the highest percentage of the report.
– these matrices had the highest percentage of MRL exceedance rates
(16% herbs and 9% tea).
• In multiresidue methods one of the main problems is the wide range

of chemical properties of the analytes. Tea leaves comprise sugars,
pigments, polyphenols and alkaloids (especially caffeine).
Objective
• The aim of the experiments was to compare and choose the best
method for the extraction of pesticides residues in tea. Three
popular extraction methods were selected for the comparison:
• modified QuEChERS with CaCl2
• ethyl acetate method
• mini-Luke
• Validate the selected method in four different matrices and apply it

to real samples.
– Green tea -Black tea
– Red Tea - Chamomile

Without
Tomato
dilution Orange
Leek
Tomato
Orange
Leek
Data base of 300 pesticides

Mass 912 components
(parent molecules, MS fragment ions and Cl isotopes)
m/z: 100-400
Rt: 7-13 min
DB: 227 components

Co-extracted matrix components of tomato. LC-TOF-MS

Mass
m/z: 200-600
2408 Matrix compounds
Rt: 4-7 min Absolute height ≥ 10000 counts
Data base components- tomato matrix compounds

Mass
m/z: 200-600 m/z: 100-400

Rt: 4-7 min Rt: 7-13 min Absolute height ≥ 10000 counts
DB: 227 components

Tomato: 656 matrix compounds
Co-extracted matrix components of green-tea. LC-TOF-MS

m/z: 100-700 Absolute height ≥ 10000 counts
Rt: 4-10 min
Data base components- green tea matrix compounds
m/z: 100-700 m/z: 100-400 9073 Matrix compounds

Absolute height ≥ 10000 counts
Rt: 4-10 min Rt: 7-13 min
DB: 227 components

Green tea: 3533 matrix compounds
Co-extracted matrix components of chamomile. LC-TOF-MS
m/z: 100-500 6630 Matrix compounds

Rt: 5-11 min
Data base components- chamomile matrix compounds
m/z: 100-500 m/z: 100-400 6630 Matrix compounds

Rt: 5-11 min Rt: 7-13 min
DB: 227 components

Chamomile: 3490 matrix compounds
Selected Compounds
86 LCa- and GCb- amenable pesticides Fungicide
Azoxystrobin a
Benalaxyl b
Insecticide Biphenylb
Acaricide
Boscalid b
Acetamiprid a
Bifenthrinb Methidathion b Carbendazim a
PGR Chlorpyrifos b
Buprofezin a Methiocarb sulfonea Cyproconazole b
Cypermethrin b
Carbaryl a Methiocarb 2,4 Da Cyprodinil b
Ethoprophos b
Carbofuran a sulfoxidea 2,4 DPa Dichlofluanid b
Etofenprox b
Chinomethionat b Methiocarba Dicloran b
Fenitrothion b
Chlorpyrifos Methyl b Methomyl a Fenarimol b
Flucythrinate b
Diazinon b Mevinphos b Fludioxonil b
Fonofos b
Dichlorvos b Monocrotophos a Imazalil a
Imidacloprid a
Dimethoate a Parathion Ethyl b Herbicide Isofenphos
Iprodione b
Endosulfan I b Phorate b Kresoxim Methyl
Methyl b b Metalaxyl a
Endosulfan II b Phosmet b Alachlor b
Lindane b
Endosulfan sulfate b Pirimiphos Methyl a Atrazine a Myclobutanil a
Parathion
Esfenvalerateb Profenofos a MCPP a Omethoate a
Methyl b
Ethion b Propargite b Metolachlor a Oxadixyl b
Permethrin b
Fenpropathrin b Pyridaben b Metribuzin a Penconazole b
Pirimicarb a
Fenvalerateb Quinalphos b Propyzamide b Pyrimethanil b
Pyriproxyfen b
Isocarbophos b Tetrachlorvinphos b Simazine a Triadimefon a
Terbufos b
Malathion b Triazophos b Terbuthylazine Triadimenol a
Thiodicarb a
a Trifluralin b Vinclozolin b
Spiking procedure
• A key aspect to achieve reliable recovery results is the

spiking process.
• Herbs are dehydrated samples, so they must be fortified
with the mix thoroughly soaking all sample, and dried
again.
Extend the tea on

Add the spiking mix Stir to be sure of the Evaporate the
the crystallizer
homogenizer solvent
procedure
Modified QuEChERS
2 g sample + 4 mL H2O
method Shake 30 sec, wait 30 min
Add 10 mL acetonitrile and
Shake automatically
200 µL TPP (25 ppm)
in Agitax
Add 4 g MgSO4 + 1 g NaCl + 1 g

NaAc·2 H2O + 0.5 g NaAc·6 H2O
Shake automatically
in Agitax
Centrifugue 5 min.
3700 r.p.m.
Take 3 mL aliquot
Add 150 mg CaCl2

anh. + 150 mg PSA
Shake 30 second
in Vortex
Centrifugue 5 min.
3700 r.p.m.
Acidify with 10 μL formic
acid 5% per mL of extract Evaporate to dryness
and reconstitute
Analysis
Modified QuEChERS
method Shake 30 sec, wait 30 min
Add 10 mL acetonitrile and
Shake automatically
200 µL TPP (25 ppm)
in Agitax
Add 4 g MgSO4 + 1 g NaCl + 1 g

NaAc·2 H2O + 0.5 g NaAc·6 H2O
Shake automatically 5 times

in Agitax dilution
Centrifugue 5 min.
3700 r.p.m.
Take 3 mL aliquot
Add 150 mg CaCl2

anh. + 150 mg PSA
Shake 30 second
in Vortex
Centrifugue 5 min.
3700 r.p.m.
Acidify with 10 μL formic
acid 5% per mL of extract Evaporate to dryness
and reconstitute
Analysis
Ethyl acetate method
Shake 30 sec, wait 30 min
Add 10 mL ethyl acetate and
Shake 3 s by hand 200 µL TPP (25 ppm)
Add 210 mg GCB +

4.8 g MgSO4
anhidrous + 0.9 g NaCl
5 times
Shake automatically
in Agitax 15 min
dilution
Centrifugue 5 min.
3700 r.p.m.
Evaporate to dryness
and reconstitute
Analysis
miniLuke
extraction method 2 g sample + 4 mL H2O
Shake 30 sec, wait 30 min
Add 10mL of Acetonitrile and
Shake vigorously 200 µL TPP (25 ppm)
30s by Ultra-Turrax
Add 20mL Petroleum ether:
Dichloromethane (1:1)
Shake vigorously
30s by Ultra-Turrax
Centrifugue 5 min.
at 4000 r.p.m.
Evaporate to dryness 3 mL
5 times portion of the upper layer
dilution
Reconstitute with 1 mL of
adecuate solvent
Analysis
LC and GC analysis
• LC analysis:
– Mobile phases: 0.1% FA in H2O and AcN
– Reversed-phase C8 analytical column of 4.6 mm x
150 mm and 5 µm particle size (Agilent Zorbax SB)
– 6410 LC-QQQ-MS/MS (Agilent Technologies)
– Dynamic MRM software features
• GC analysis:
– Ultra Inert GC column, HP-5MS UI 15 m × 0.25 mm
i.d. × 0.25 μm (Agilent)
– 7000 GC-QQQ-MS/MS (Agilent Technologies)
– Retention Time Locking (RTL) and Blackflushing
– 39 segment SRM method
Recoveries
50
45
40
35
30
# Compounds
25 QuEChERS
20
15 EtOAc
10
miniLuke
5
0
0-30 30-
40- 50-
40 50 60- 70-
60 70 80- 90-
80 90 100- n.d.
100 120
Recovery (%)
Concentration level: 100 µg/kg (n=5)
Recoveries
Number of compounds
Ethyl Acetate
QuEChERS miniLuke
method
70 - 120% 75 31 54
70 - 60% 2 26 26
< 60% 6 22 2
Not detected 3 7 4
Lowest recoveries with modified QuEChERS method
Pvap pKow modified QuEChERS

Compound (Pa, 20ºC) (pH 7, 20ºC) Rec (%) RSD(%)
Ometoathe a 3,3·10-03 -0,74 19,8 15,3
Monocrotophos a 2,9·10-04 -0,22 34,0 12,6
MCPA a 4,0·10-04 -0,81 45,5 19,3
2,4-D a < 1,0·10-05 -0,83 46,6 22,8
Dichlofluanid b* 1,4·10-05 3,70 49,4 8,3
Dicamba a 1,7·10-03 -1,88 51,7 15,9
Carbendazim a 1,5·10-04 1,48 56,9 17,2
a Ansalysed by LC
b Ansalysed by GC
* Thermical degradation into the GC system
CaCl2
Lowest recoveries with ethyl acetate method
Pvap pKow EtOAc method Pvap pKow EtOAc method

Compound (Pa, 20ºC) (pH 7, 20ºC) Rec (%) RSD(%) Compound (Pa, 20ºC) (pH 7, 20ºC) Rec (%) RSD(%)
Cyprodinil b 5,1·10-04 4,00 0,0 0,0 Thiodicarb a 2,7·10-03 1,62 51,6 6,6
Pirimiphos Methyl a 2,0·10-03 3,90 31,1 9,9 Metolachlor a 4,2·10-04 3,40 51,9 6,8
Imazalil a 1,6·10-04 2,56 31,9 7,1 Kresoxim Methyl b 2,3·10-06 3,40 52,7 3,5
Chinomethionat b 2,6·10-05 3,78 33,1 8,7 Fenarimol b 6,5·10-05 3,69 53,1 2,0
Ometoathe a 3,3·10-03 -0,74 37,4 6,3 Penconazole b 3,7·10-04 3,72 53,1 2,6
Terbufos b 3,5·10-02 4,51 37,7 16,4 Iprodione b 5,0·10-07 3,10 54,8 4,2
Boscalid b 7,0·10-07 2,96 39,3 5,3 Alachlor b 2,0·10-03 3,09 55,5 6,8
Terbuthylazine a 1,5·10-04 3,40 44,4 6,7 Isofenphos Methyl b 4,04 55,9 4,1
Diazinon b 1,2·10-02 3,69 46,3 7,6 Malathion b 4,5·10-04 2,75 56,8 3,5
Azoxystrobin a 1,1·10-10 2,50 47,1 6,7 Fludioxonil b 3,9·10-07 4,12 56,9 3,3
Pyrimethanil a 1,1·10-03 2,84 48,4 10,3 Quinalphos b 3,5·10-04 4,44 57,4 4,0
Myclobutanil a 2,1·10-04 2,89 48,4 6,1 Fonofos b 2,8·10-02 3,94 57,7 14,5
Phorate b 8,5·10-02 3,86 48,7 3,8 Benalaxyl b 6,6·10-04 3,54 58,2 4,8
a Ansalysed by LC Vinclozolin b 1,3·10-04 3,02 59,0 6,4
b Ansalysed by GC
GCB
Green Tea Blank

LC-QToF-MS Full Scan Total Ion Chromatogram
Mini Luke method

EtOAc method
QuEChERS method
Green Tea Blank

GC-Q-MS Full Scan Total Ion Chromatogram
Mini Luke method

EtOAc method
QuEChERS method
Set-up
Green tea
Modified QuEChERS Ethyl Acetate method miniLuke method
Chamomile
Validation in 4 different matrices Green tea
with the best method Red Tea
Black tea
Set-up
Green tea
Modified QuEChERS Ethyl Acetate method miniLuke method
Chamomile
Validation in 4 different matrices Green tea
with the best method Red Tea
Black tea
Recoveries
Concentration level: 25 μg/Kg (n=5)
50
45
40
Compounds (%)
35
30 Green Tea
25 Red Tea
20 Black Tea
Camomile
15
10
5
0
Recovery (%)
Recoveries
50
45
40
Compounds (%)
35
30 Green Tea
25 Red Tea
20 Black Tea
Camomile
15
10
5
0
Recovery (%)
Recoveries
60
55
50
45
Compounds (%)
40
Green Tea
35
30 Red Tea
25 Black Tea
20 Chamomile
15
10
5
0
Recovery (%)
Recoveries
60
55
50
45
Compounds (%)
40
Green Tea
35
30 Red Tea
25 Black Tea
20 Chamomile
15
10
5
0
Recovery (%)
Benalaxyl
LODs Cypermethrin
Fonofos
Quinalphos
Profenofos
45
40 Fonofos
Compounds (%)
35 Mevinphos
30
25
20
Green tea
15
10
Red Tea
5 Black Tea
0 Chamomile
0,1-0,25 0,25-0,5 0,5-1 1-5 5-10 10-50 50-100 > 100
LOD (μg/kg) Quinalphos Mevinphos
Propargite
Linearity and repetitivity
• Linearity
– 7 calibration points, 0,5-200 μg/L
– All the compounds had a R2>0.99
• Repetitivity
– Two concentration levels: 5 and 20 μg/L
– RSD<17%
Matrix effects
18
16
14
Compounds (%)
12
10
Green tea
8 Red Tea
6 Black Tea
4 Chamomile
2
0
< -50% -50% - -20% - 0- 20% - 50% - 100% - 200% - 300% - 400% - >
(-20%) 0 20% 50% 100% 200% 300% 400% 500% 500%
Slope Variation (%)

Blank matrices extracted with modified QuEChERS method

Blank matrices extracted with modified QuEChERS method

Real samples
75 real samples of different kind of herbs bought in:
26 samples 26 samples 9 samples
6 samples 3 samples
1 sample 1 sample 1 sample
1 sample 1 sample
Real samples
Results
8.0%
24.0%
68.0%
Under MRL Above MRL Blank
Uncertainty of 50% is considered to

check the MRL exceedance.
Real samples
Distribution of the pesticides in the samples
12
10
8
# Samples
0
0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15
# Pesticides
Real samples
Distribution of the pesticides in the samples
12
10
8
# Samples
0
0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15
# Pesticides
Most found: Biphenyl (37), Acetamiprid (36), Carbendazim (36), Chlorpyrifos (34),
Imidacloprid, (31), Bifenthrin (30) and Endosulfan (Sum) (22).
APPLICATION TO REAL SAMPLES

SAMPLE PESTICIDE DETECTED CONCENTRATION (μg/Kg)
Acetamiprid 20.9
Bifenthrin 39.2
Red tea_1 Biphenyl 13.0
Carbendazim 15.4
Imidacloprid 15.9
Carbendazim 220.2
Carbofuran 11.8
Chlorpyrifos 15.8
Chamomille_3 Endosulphan I 6.0
Metalaxyl 6.0
Etofenprox 18.3
Penconazole 7.1
Acetamiprid 106.2
Bifenthrin 168.5
Carbendazim 15.6
Endosulphan I 19.0
Green tea_5
Endosulphan II 34.1
Endosulphan sulphate 38.2
Imidacloprid 38.9
Methomyl 15.4
Acetamiprid 29.1
Bifenthrin 136.5
Carbendazim 2.6
Black tea_10 Endosulphan I 18.3
Endosulphan II 43.6
Imidacloprid 26.9
In red, values above MRL


DETECTED CONCENTRATION DETECTED CONCENTRATION
SAMPLE SAMPLE
PESTICIDE (μg/Kg) PESTICIDE (μg/Kg)
Acetamiprid 271.0 Acetamiprid 15.6
Bifenthrin 328.7 Biphenyl 7.2
Biphenyl 20.0 Black tea_41 Carbendazim 43.0
Carbendazim 14.0 Methiocarb sulfone 21.2
Carbofuran 7.7 Pyridaben 4.9
Clorpyrifos 45.9
Acetamiprid 13.3
Endosulphan I 34.7
Green tea_34 Bifenthrin 81.9
Endosulphan II 112.7
Buprofezin 1.3
Endosulphan sulphate 111.1 Black tea_57
Chlorpyrifos 4.5
Fenpropathrin 33.6
Imidacloprid 7.6
Imidacloprid 124.9
Methiocarb Sulfone 7.6
Methomyl 36.5
Pyridaben 2.9 Acetamiprid
Triazophos 21.7 29.1
Bifenthrin
136.5
Carbendazim
Acetamiprid 112.7 2.6
Endosulphan I
Bifenthrin 235.0 Black tea_10 18.3
Endosulphan II
Biphenyl 19.2 43.6
Endosulphan
Carbaril 16.1 70.6
sulphate
Carbendazim 19.8 26.9
Imidacloprid
Clorpyrifos 6.6
Green tea_35 Endosulphan I 9.7 Acetamiprid 26.7
Endosulphan II 40.8 Biphenyl 13.9
Endosulphan sulphate 42.2 Carbendazim 19.3
Fenpropathrin 60.9 Black tea_21 Chlorpyrifos 3.2
Imidacloprid 116.6 Imidacloprid 61.6
Methomyl 12.7 Methiocarb sulfone 20.5
Triazophos 6.9 Pyridaben 3.2


Acetamiprid 20.1
Bifenthrin 55.2
Carbaril 11.8
Carbendazim 6.8
Green tea_9 Endosulphan I 13.9
Imidacloprid 35.1
Methomyl 3.9
Propargite 44.1
Acetamiprid 29.1
Bifenthrin 136.5
Carbendazim 2.6
Black tea_10 Endosulphan I 18.3
Endosulphan II 43.6
Imidacloprid 26.9
Acetamiprid 217.2
Bifenthrin 478.3
Buprofezin 75.3
Carbendazim 33.6
Carbofuran 1.9
Chlorpyrifos 16.1
Endosulfan I 25.3
Green tea_75 Endosulfan II 100.0
Endosulfan suphate 114.0
Imidacloprid 118.4
Fenvalerate/Esfenvalerate RR/SS 56.8
Fenvalerate/Esfenvalerate RS/SR 63.5
Methomyl 49.7
Pyridaben 10.8
Triazophos 39.0

Carbendazim 5.2
Chlorpyrifos 18.7
Etofenprox 29.3
Rooibos tea_19
Imazalil 41.2
Iprodione 0.6
Methomyl 4.4
Biphenyl 9.9
Boscalid 32.4
Carbendazim 30.0
Carbofuran 3.7
Chlorpyrifos 73.9
Herbs and fruits_23 Fludioxonil 20.2
Iprodione 64.6
Pirimetanil 46.5
Pirimicarb 2.7
Propargite 278.2
Pyrimethanil 78.7
Pyrimiphos methyl 1.7
Acetamiprid 45.7
Bifenthrin 105.0
Biphenyl 21.1
Carbendazim 10.6
Chlorpyrifos 6.6
Endosulphan I 10.2
Black-green tea_30
Endosulphan II 37.0
Imidacloprid 52.4
Methomyl 3.8
Monocrothophos 10.3
Triazophos 7.8
Conclusions
• From the three MRM the preferred method for the analysis of
pesticides residues in green tea was QuEChERS with calcium
chloride. This method was the best in terms of recoveries and the
full scan chromatograms were the least influenced with coextracted
matrix compounds.
• The method was validated studying recoveries, limits of detection,

linearity , repeatability and matrix effects, with good results.
• It was applied to real samples from different countries, where 92% of

them were positives, as average they contained 5 pesticides per
sample and 24% exceeded the EU MRL.
Tea infusion
Infusion for LC analysis
2 g sample
50mL of boiled
milliQ water
Stir during 15 min
Take 900µL of
infusion + 100µL of
acetonitrile
27.8
times
Filter dilution
Analysis by
LC-MS/MS
Transfer (%) of the pesticides from the leaves to the infusion
Water solubility
Ring Test Tea

Results
Participating labs
1 1
1
1 Number of participating labs in each country

Preparation of test material

Results
EU and
EU EU Lab 2
Lab 1 Lab 3 Lab 4 Lab 5 EURL- Lab 6 Lab 7 3rd
Compound Average RSD (Sri
(France) (Sweden) (Germany) (Austria) FV (Thailand) (Thailand) Countries
(mg/kg) (%) Lanka)
RSD (%)
Acetamiprid 0.565 0.583 0.517 0.647 0.606 0.584 8.3 0.567 0.582 6.9
Bifenthrin 0.392 0.683 NA 0.711 0.634 0.605 24.1 0.402 0.801 28.0
Buprofezin 0.043 0.116 0.142 0.108 0.102 41.2 0.098 0.078 34.9
Carbofuran 0.022 0.016 0.027 0.022 26.3 Detected 26.3
Chlorpyrifos 0.014 0.013 0.009 0.012 20.8 Detected NA 20.8
Cypermethrine 0.065 NA 0.113 0.089 38.1 Detected 0.067 NA 33.2
Endosulfan Alpha 0.047 0.099 NA 0.087 0.100 0.083 29.8 0.079 1.781 189.8
Endosulfan Beta 0.077 0.183 NA 0.126 0.171 0.139 34.6 0.506 0.704 85.4
Endosulfan Sulfate 0.088 0.072 NA 0.049 0.080 0.072 23.3 NA 0.086 0.072 19.0
Fenpropathrin 0.090 0.193 NA 0.182 0.200 0.166 30.9 0.281 NA 0.219 32.0
Fenvalerate 0.031 0.050 NA 0.059 0.050 0.047 30.6 Detected 0.038 28.0
Imidacloprid 0.115 0.079 0.077 0.136 0.120 0.105 24.9 0.111 NA 22.2
Methomyl 0.231 0.278 0.388 0.345 0.311 22.5 NA NA 0.327 19.4
Pyridaben NA 0.024 0.024 0.095 84.0
Triazophos 0.028 0.042 0.044 0.033 0.037 20.4 0.219 0.015 121.0
Concentration expressed as mg/kg

NA: Not Analised
Concentration (mg/kg)
0
0.1
0.2
0.3
0.4
0.5
0.6
0.7
0.8
Acetamiprid
Bifenthrin
Lab 1 (France)
Buprofezin
Carbofuran
Chlorpyrifos
Lab 3 (Sweden)
Cypermethrine
Endosulfan Alpha
Endosulfan Beta
Lab 4 (Germany)
Endosulfan Sulfate
Fenpropathrin
Imidacloprid
European labs results
Lab 5 (Austria)
Methomyl
Pyridaben
EURL-FV
Triazophos
Fenvalerate
Thank You
for Your Attention

Analysis of Pesticides

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Analysis of Pesticides

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Interested in conducting your own webinar? Email webinars@bnpmedia.

Analysis of pesticides in herbs

• The EFSA annual report of 2008 revealed that:

• In multiresidue methods one of the main problems is the wide range

• Validate the selected method in four different matrices and apply it

– Red Tea - Chamomile

Data base of 300 pesticides

DB: 227 components

Co-extracted matrix components of tomato. LC-TOF-MS

Data base components- tomato matrix compounds

m/z: 200-600 m/z: 100-400

DB: 227 components

Co-extracted matrix components of green-tea. LC-TOF-MS

9073 Matrix compounds

Data base components- green tea matrix compounds

m/z: 100-700 m/z: 100-400 9073 Matrix compounds

DB: 227 components

Co-extracted matrix components of chamomile. LC-TOF-MS

m/z: 100-500 6630 Matrix compounds

Data base components- chamomile matrix compounds

m/z: 100-500 m/z: 100-400 6630 Matrix compounds

DB: 227 components

• A key aspect to achieve reliable recovery results is the

Extend the tea on

Add 4 g MgSO4 + 1 g NaCl + 1 g

Add 150 mg CaCl2

Add 4 g MgSO4 + 1 g NaCl + 1 g

Shake automatically 5 times

Add 150 mg CaCl2

Ethyl acetate method

Add 210 mg GCB +

Lowest recoveries with modified QuEChERS method

Pvap pKow modified QuEChERS

Lowest recoveries with ethyl acetate method

Pvap pKow EtOAc method Pvap pKow EtOAc method

Green Tea Blank

Mini Luke method

Green Tea Blank

Mini Luke method

Modified QuEChERS Ethyl Acetate method miniLuke method

Modified QuEChERS Ethyl Acetate method miniLuke method

Linearity and repetitivity

Slope Variation (%)

Blank matrices extracted with modified QuEChERS method

Blank matrices extracted with modified QuEChERS method

26 samples 26 samples 9 samples

1 sample 1 sample 1 sample

Under MRL Above MRL Blank

Uncertainty of 50% is considered to

APPLICATION TO REAL SAMPLES

In red, values above MRL

APPLICATION TO REAL SAMPLES

In red, values above MRL

APPLICATION TO REAL SAMPLES

APPLICATION TO REAL SAMPLES

• The method was validated studying recoveries, limits of detection,

• It was applied to real samples from different countries, where 92% of

Infusion for LC analysis

Transfer (%) of the pesticides from the leaves to the infusion

Ring Test Tea

1 Number of participating labs in each country

Preparation of test material

Concentration expressed as mg/kg

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